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N-methyl piperazine and N-ethyl piperazine separation method

A technology of ethylpiperazine and methylpiperazine, which is applied in the field of separation and purification of fine chemicals, can solve the problems of failure to meet the separation requirements and difficulties in meeting the separation requirements, and achieve solvent recycling, high purity, and simple operation process Effect

Active Publication Date: 2014-11-05
XIAN MODERN CHEM RES INST
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  • Abstract
  • Description
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Problems solved by technology

[0004] N-methylpiperazine is similar to N-ethylpiperazine boiling point, is difficult to reach separation requirement by common rectification, the inventor adopts rectification tower to separate N-methylpiperazine and N-ethylpiperazine, The theoretical plate number of the rectification column is 20 plates, the reflux ratio is 5:1, and the purity of N-methylpiperazine at the top of the tower is about 70%, which does not meet the separation requirements

Method used

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  • N-methyl piperazine and N-ethyl piperazine separation method

Examples

Experimental program
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Effect test

Embodiment 1

[0016] Push the crude material N-methylpiperazine and N-ethylpiperazine into the extraction tower B3 with the crude product feed pump B2, the feed position is at 20 theoretical plates, and the extractant N-hydroxyethylethylenediamine is used The extraction agent feed pump B1 enters the extraction tower B3, the feeding position is at 5 theoretical plates, the mass ratio of the extractant to the crude material is 0.5:1, and the number of theoretical plates of the extraction tower is not less than 30 theoretical plates , the reflux ratio is 10:1, the operating pressure is 0.1atm, N-methylpiperazine is extracted from the top of the tower, and the material in the bottom of the extraction tower is pumped into the solvent recovery tower B4 with the pump B5 at the bottom of the extraction tower, and the feeding position is 15 blocks At the theoretical plate, the number of theoretical plates of the solvent recovery tower is not less than 30 theoretical plates, the reflux ratio is 10:1, ...

Embodiment 2

[0018] The same operation as in Example 1, the feed position of the crude material is the 23rd theoretical plate, the extractant is N-hydroxyethylpiperazine, the feed position is the 8th theoretical plate, the extractant and the crude material The mass ratio of the extraction tower is 2:1, the number of theoretical plates of the extraction tower is 35, the reflux ratio is 5:1, the operating pressure is 0.5 atm, the feed position of the extraction tower tank material is the 18th theoretical plate, and the solvent recovery tower The number of theoretical plates is 35, the reflux ratio is 5:1, the operating pressure is 0.5atm, and the temperature of the extractant after cooling is 35°C. The purity of N-methylpiperazine and N-ethylpiperazine determined by gas chromatography was 99.0% and 99.2%, respectively.

Embodiment 3

[0020] The same operation as in Example 1, the crude feed position is the 25th theoretical plate, the extractant is N-hydroxyethylethanolamine, and the feed position is the 10th theoretical plate, the extractant and crude material The mass ratio is 3:1, the number of theoretical plates of the extraction tower is 40, the reflux ratio is 1:1, the operating pressure is 1 atm, the feed position of the extraction tower tank material is at the 20th theoretical plate, and the solvent recovery tower theoretical column The number of plates is 40, the reflux ratio is 1:1, the operating pressure is 1 atm, and the temperature of the extractant after cooling is 50°C. The purity of N-methylpiperazine and N-ethylpiperazine determined by gas chromatography was 99.7% and 99.8%, respectively.

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Abstract

The invention discloses a N-methyl piperazine and N-ethyl piperazine separation method. According to the method, an extraction agent is used for separation of N-methyl piperazine and N-ethyl piperazine in an extraction tower, the N-methyl piperazine is collected at the tower top, a tower kettle material is pump into a solvent recovery tower by an extraction tower kettle bottom pump, the N-ethyl piperazine is collected at the tower top of the solvent recovery tower, and the extraction agent is collected from a side line, and is condensed to go back to the extraction tower for circular use. The method is used for the separation of the N-methyl piperazine and the N-ethyl piperazine.

Description

technical field [0001] The invention belongs to the technical field of separation and purification of fine chemicals, and relates to a method for separating N-methylpiperazine and N-ethylpiperazine. Background technique [0002] N-methylpiperazine and N-ethylpiperazine are important derivatives of piperazine. N-methylpiperazine is widely used in medicine, surfactants, synthetic fibers, etc., and is also an important intermediate in organic synthesis; N-methylpiperazine is a new generation of broad-spectrum antibacterial drug ofloxacin It is also used as an intermediate of clozapine to synthesize dyes and pesticides, and is also widely used in polymer materials such as plastics and rubber. N-ethylpiperazine is mainly used in the synthesis of enrofloxacin, dyes and plant protection agents, etc. It is also widely used in polymer industries such as plastics and rubber. It can also be used as a human insecticide and antibiotic. Raw materials for repelling roundworms and burning...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/023C07D295/03
CPCC07D295/023C07D295/03
Inventor 李亚妮吕剑王伟杨建明徐强王为强赵峰伟
Owner XIAN MODERN CHEM RES INST
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